HRID2223875
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 2-(1-benzylpiperidin-4-ylamino)-5-methylpyridine (11.3 g) in ethanol (250 mL) was added 20% palladium hydroxide (4 g). After stirring the solution at room temperature under hydrogen atmosphere for 48 hours, 20% palladium hydroxide (2 g) was further added. The solution was then stirred at room temperature under hydrogen atmosphere for additional 99 hours. The catalyst was filtered off. After concentration under reduced pressure, the resulting residue was purified by chromatography [NH silica gel, chloroform:methanol=10:1]. The resulting crude product was crystallized from ethyl acetate/hexane to give the title compound (5.97 g).
WORKUP
后处理
- stirringThe solution was then stirred at room temperature under hydrogen atmosphere for additional 99 hours
- filtrationThe catalyst was filtered off
- concentrationAfter concentration under reduced pressure
- customthe resulting residue was purified by chromatography [NH silica gel, chloroform:methanol=10:1]
- customThe resulting crude product was crystallized from ethyl acetate/hexane